CN111624277A - Full-automatic comprehensive sample pretreatment instrument - Google Patents
Full-automatic comprehensive sample pretreatment instrument Download PDFInfo
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- CN111624277A CN111624277A CN202010265533.8A CN202010265533A CN111624277A CN 111624277 A CN111624277 A CN 111624277A CN 202010265533 A CN202010265533 A CN 202010265533A CN 111624277 A CN111624277 A CN 111624277A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention relates to a full-automatic comprehensive sample pretreatment instrument which comprises a sampling module, a cleaning module, a processing module, a lofting module, a collecting module, a column temperature control module, an extraction sample introduction module and an operation control module. The invention can select the functions of eliminating, purifying, extracting, enriching, desorbing and separating the on-line/off-line matrix of the used sample by switching the control circuit and the valve, and each function of the invention can be independently used on-line/off-line and also can be randomly combined and used according to the requirement, thereby realizing the purpose of converting the sample of the complex matrix into the target sample; the method reduces or removes interferents, concentrates and enriches components to be detected, reduces the influence of a complex sample on an analysis result, further meets the requirement of a target object on chromatographic separation analysis, improves the response value of instrument detection, avoids errors caused by manual pretreatment, and ensures the repeatability and accuracy of instrument test. The invention is suitable for the fields of medicine and health, environmental protection, food detection, scientific research and industrial wastewater detection.
Description
Technical Field
The invention relates to the field of pretreatment of analytical chemical samples, in particular to a full-automatic comprehensive sample pretreatment instrument which is suitable for online/offline matrix elimination, purification, extraction, enrichment, desorption and separation of trace compounds in samples in the fields of medicine and health, environmental protection, food detection, scientific research, industrial wastewater detection and the like.
Background
For the detection and analysis of complex matrix samples, pretreatment is generally required, such as off-line or on-line separation and enrichment of target analytes in the samples by using various extraction materials, and then injection into a chromatographic system for analysis, most commonly solid-phase extraction. However, the offline solid-phase extraction method needs to concentrate and sample the sample manually, and the time for loading the sample and processing the sample by the solid-phase extraction cartridge is long, so that the whole analysis time is prolonged, different reagents need to be replaced, the work intensity and time of an experimenter are increased by frequent operation, the manual operation is complicated, the contact between people and potential infectious substances is large, and the detection safety is poor; the traditional on-line solid phase extraction column method can only extract the target object in a cleaner sample in a large volume (such as a water sample), and cannot extract the target object in a large volume (such as a blood sample) in a complex sample.
Disclosure of Invention
The invention aims to overcome the defects that complex samples cannot be eliminated, purified, extracted, enriched, desorbed and separated on an online matrix, and designs a pretreatment system which can realize the combination of offline solid-phase extraction and online solid-phase extraction of complex matrix samples, so that a target object can be directly separated and analyzed in a chromatogram after full-automatic pretreatment, the test process does not need manual participation, and all modules are mutually matched to realize the full-flow work from sample introduction to result output.
The technical scheme adopted by the invention for solving the technical problem is as follows:
the utility model provides a full-automatic preceding processing apparatus is synthesized to sample, includes the casing, be provided with sampling module on the casing, wash the module, processing module, lofting module, collection module, post temperature control module, extraction advance kind module and operation control module.
The casing includes shrouding, sample dish upper seal board, side shrouding and frame before the sample dish.
The lofting module comprises a sample disc base plate, a sample disc and a sample disc upper fixing plate, wherein the sample disc base plate is arranged on the shell, the sample disc is rotatably arranged on the sample disc base plate, and the sample disc upper fixing plate is arranged at the upper end of the sample disc.
The sampling module is arranged on the upper sealing plate of the sample disc at one side of the sample disc and comprises a sampling needle, a sampling needle swing arm and a rotary arm motor; the first rotating motor is installed inside the shell, a sampling needle swing arm is installed on a rotating shaft of the first rotating motor, and a sampling needle is installed on the sampling needle swing arm.
The cleaning module is arranged on the sample plate upper sealing plate on one side of the sample plate and comprises a needle washing station and a needle washing bottle.
Processing module installs on the sample dish of sample dish one side goes up the shrouding, processing module includes SPE column pressure head, pressure head swing arm and second rotation motor, the second rotates the motor and installs inside the casing, install the pressure head swing arm in the pivot that the second rotated the motor, SPE column pressure head is installed to pressure head swing arm upper end.
The collection module is mounted on the sample tray chassis and includes a collection trough.
The temperature control column module is arranged on the front sealing plate side of the foreign product tray and comprises a column temperature control cover plate and a column temperature control fixing groove.
The extraction advances kind module and installs in the right side of casing, the extraction advances kind module and includes high-pressure extraction pump, sampling valve, first three-way valve, second three-way valve, high-pressure reagent pump, multi-way diverter valve, first sample extraction valve, second sample extraction valve, sample transfer valve.
The operation control module comprises a touch display and a controller mainboard, the touch display is mounted at the front end of the shell, and the controller mainboard and the side sealing plate are connected inside the shell.
The shell is further connected with a first serial port adapter, a second serial port adapter, a connector and an IC card reader of the power socket.
A pretreatment method of a full-automatic sample comprehensive pretreatment instrument comprises the following steps:
placing the sample tube, the extraction tube and the collection tube in a designated station of the lofting module in sequence, and setting corresponding processing methods in the operation control module in sequence;
the sampling module quantitatively sucks a sample from a sample tube in the lofting module to a designated processing station (extraction tube); before different samples are sucked, the cleaning module cleans the sampling module;
the processing module quantitatively releases the reagent to a designated processing station (extraction tube), and after incubation for a certain time, the air pump positive pressure extraction tube is started to transfer the processed target solution to the collection module; wherein, the types of the reagents are one or more; before different reagents are sucked, the cleaning module cleans the processing module;
the collection module collects and quantitatively transfers the target solution to a quantitative ring of a sample injection valve in the extraction sample injection module; cleaning the collection module after transferring;
the extraction and sample introduction module is used for carrying out on-line further treatment on the target solution transferred by the collection module, including further purification, extraction, enrichment, desorption and separation, and the treated solution can be directly transferred into an on-line analysis column.
A sampling module: the sampling module is used for sucking a sample and transmitting the sample to a specified processing station;
a cleaning module: the cleaning module is used for cleaning the sampling module and the processing module;
a processing module: the processing module is used for absorbing the reagent and transmitting the reagent to a designated processing station; the device is also used for transferring the mixed solution of the sample and the reagent into a collection module through positive pressure filtration of an air pump;
a lofting module: the lofting module is used for placing a sample tube, an extraction tube and a collection bottle; the temperature control device is also used for controlling the temperature of the sample in the whole pretreatment process;
a collection module: the collecting module is used for collecting and transferring the target solution after the treatment of the treatment module; the device is also used for collecting and transferring the waste liquid treated by the treatment module;
column temperature control module: the column temperature control module is used for controlling and protecting the temperature of the on-line extraction column and the chromatographic analysis column;
an extraction sample introduction module: the extraction and sample introduction module is used for collecting the on-line further treatment of the target solution transferred by the module, including further purification, extraction, enrichment, desorption and separation;
the operation control module: the operation control module is used for setting the operations of sample processing method, instrument maintenance, operation tracking and the like.
The full-automatic sample comprehensive pretreatment instrument utilizes a sampling module, a processing module and a lofting module to realize automatic reagent adding and automatic sample treatment according to tested items, utilizes a cleaning module to clean the sampling module and the processing module so as to avoid cross contamination, utilizes an extraction sample introduction module to carry out on-line solid phase extraction on a treated sample, further purifies the sample, extracts, enriches, desorbs and separates the sample, utilizes an operation control module to carry out program setting and automatic operation on sample treatment and direct sample introduction, does not need manual participation in the test process, and is matched with each other among the modules, thereby realizing the full-flow work from sample introduction to result output.
The invention can select the functions of eliminating, purifying, extracting, enriching, desorbing and separating the on-line/off-line matrix of the used sample by switching the control circuit and the valve, and each function of the invention can be independently used on-line/off-line and also can be randomly combined and used according to the requirement, thereby realizing the purpose of converting the sample of the complex matrix into the target sample; the method reduces or removes interferents, concentrates and enriches components to be detected, reduces the influence of a complex sample on an analysis result, further meets the requirement of a target object on chromatographic separation analysis, improves the response value of instrument detection, avoids errors caused by manual pretreatment, and ensures the repeatability and accuracy of instrument test. The invention is suitable for the fields of medicine and health, environmental protection, food detection, scientific research and industrial wastewater detection.
Drawings
FIG. 1 is a schematic diagram of a fully automatic sample comprehensive pretreatment apparatus according to the present invention;
FIG. 2 is a schematic top view of the fully automatic integrated pre-treatment apparatus for specimens shown in FIG. 1 without a protective cover;
FIG. 3 is a schematic view of a collection tank of the fully automatic sample comprehensive pretreatment apparatus;
fig. 4 is a schematic top view of a lofting module in a fully automatic sample comprehensive pretreatment apparatus.
Reference numerals
1, sampling swing arm
2, sampling needle
3, SPE column pressure head
4, SPE column pressure head swing arm
5, sample plate upper sealing plate
6, sample plate
7, fixing plate on sample plate
8, front sealing plate of sample plate
9, column temperature control module
10, extraction sample introduction module
11, high pressure extraction pump
12, sample injection valve
13, first three-way valve
14, high pressure reagent pump
15, second three-way valve
16, multiple-way switching valve
17, first sample extraction valve
18, second sample extraction valve
19, sample transfer valve
20, power socket
21, first serial port adapter
22, second serial port adapter
23, connector
24, IC card reader
25, touch display
26, side sealing plate
27, controller motherboard
28, frame
29, needle washing bottle
30, needle washing station
31, collecting tank
32, sample tray chassis
Detailed Description
In order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easy to understand, the invention is further described with reference to the figures and the specific embodiments.
Example 1
Fig. 1 is a schematic diagram of a fully automatic sample comprehensive pretreatment instrument according to the present invention. Referring to fig. 1, it can be seen that sampling swing arm 1, sampling needle 2, SPE column pressure head 3, SPE column pressure head swing arm 4, sample tray upper sealing plate 5, sample tray 6, sample tray upper fixing plate 7, sample tray front sealing plate 8, column temperature control module 9, extraction sample injection sealing plate 10, high-pressure extraction pump 11, sample injection valve 12, first three-way valve 13, high-pressure reagent pump 14, second three-way valve 15, multi-way switching valve 16, first sample extraction valve 17, second sample extraction valve 18, sample transfer valve 19, power socket 20, first serial port adapter 21, second serial port adapter 22, connector 23, IC card reader 24, touch display 25, side sealing plate 26, controller motherboard 27, and frame 28. In the figure, a sampling needle 2 is arranged on a sampling swing arm 1 and is lifted and rotated along with the sampling swing arm 1; SPE column pressure head 3 is installed on SPE column pressure head swing arm 4, goes up and down and rotates along with SPE column pressure head swing arm 4. The sample plate 6 can be integrally rotated by 360 degrees around the center after being pressed and fixed by the sample plate upper fixing plate 7. The column temperature control module 9 and the sample plate front sealing plate 8 are in the same vertical surface and can be opened through the handle hole. The sample injection valve 12, the first three-way valve 13, the second three-way valve 15 and the multi-way switching valve 16 are fixed on the extraction sample injection sealing plate 10. The high-pressure extraction pump 11 and the high-pressure reagent pump 14 are fixed on the bottom plate of the frame 28, and the head part extends out of the outer surface of the extraction and sample injection sealing plate 10. The first sample extraction valve 17, the second sample extraction valve 18 and the sample transfer valve 19 are arranged above the extraction and sample injection sealing plate 10, and can be pulled out manually and disassembled and assembled quickly. The power socket 20, the first serial adapter 21, the second serial adapter 22, the connector 23, and the IC card reader 24 are mounted on the side cover plate 26. A touch display 25 is mounted on the frame 28 and an operator can manually touch the operating instrument. The controller mainboard 27 is installed on the top plate of the frame 28, and the controller slot extends out of the surface of the side sealing plate 26, so that an operator can conveniently plug and pull out external connection equipment.
Fig. 2 is a schematic top view of the fully automatic sample comprehensive pretreatment apparatus without a protective cover. The needle wash bottle 29, the needle wash station 30 can be seen. The needle washing bottle 29 and the needle washing station 30 are arranged on the bottom plate of the frame 28, and the top part of the needle washing bottle is exposed out of the surface of the upper closing plate 5 of the sample plate.
FIG. 3 is a schematic view of a collection tank of the fully automatic sample comprehensive pretreatment apparatus. The collection trough 31 can be seen mounted on a sample tray chassis 32. The collecting tank is used for recovering the filtered liquid, and the filtered liquid is recovered to a specific container through a pipeline.
Fig. 4 is a schematic top view of a lofting module in a fully automatic sample comprehensive pretreatment apparatus. The sample tray 6 in the sample placing mold is used for placing containers such as test tubes.
According to the embodiment of the invention, the sampling swing arm 1 drives the sampling needle 2 to perform lifting and rotating motion, so as to perform corresponding liquid sampling, and then the sampling needle rotates to the needle washing bottle 29 from the corresponding position of the sample disc 6; after the sampling needle 2 is washed in the needle washing bottle, the needle washing bottle is rotated to the needle washing station 30, and the sampling needle 2 is washed again. The SPE column pressing head swing arm 4 drives the SPE column pressing head 3 to perform lifting and rotating motion, firstly pressing the SPE column at the corresponding position of the sample plate 6, and performing liquid injection pressurization filtration; then, the needle washing station 30 is rotated to discharge the residual liquid in the pressure head. The filtered solution is collected by a collecting tank 31 and quantitatively transferred to a quantitative ring of a sample injection valve 12 in an extraction sample injection module; the collection tank 31 is cleaned after the solution transfer. The sample tray 6 can rotate around the center to rotate the placed sample tubes, extraction tubes and collection bottles to corresponding positions. The column temperature control module 9 is used for controlling and protecting the temperature of the on-line extraction column and the chromatographic analysis column, and the external cover plate can be manually and rapidly opened.
According to the embodiment of the invention, the extraction and sample injection module is composed of an extraction and sample injection closing plate 10, a high-pressure extraction pump 11, a sample injection valve 12, a first three-way valve 13, a high-pressure reagent pump 14, a second three-way valve 15, a multi-way switching valve 16, a first sample extraction valve 17, a sample extraction valve 18 and a sample transfer valve 19. The extraction and sample introduction module is used for on-line further processing of the target solution transferred by the collection module 31, including further purification, extraction, enrichment, desorption and separation. The power socket 20 is provided with a filtering switch and is externally connected with a 220V power supply for supplying power to the instrument. The first serial adapter 21, the second serial adapter 22 and the connector 23 are used for external instrument connection. The IC card reader 24 is used for card reading identification. The touch display 25 is used for an operator to perform operations such as corresponding settings. The controller mainboard 27 is used for all data operation and storage of the instrument.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, and that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (12)
1. The utility model provides a preceding processing appearance is synthesized to full-automatic sample, includes the casing, its characterized in that: the shell is provided with a sampling module, a cleaning module, a processing module, a lofting module, a collecting module, a column temperature control module, an extraction sample introduction module and an operation control module.
2. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: the casing includes shrouding, sample dish upper seal board, side shrouding and frame before the sample dish.
3. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: the lofting module comprises a sample disc base plate, a sample disc and a sample disc upper fixing plate, wherein the sample disc base plate is arranged on the shell, the sample disc is rotatably arranged on the sample disc base plate, and the sample disc upper fixing plate is arranged at the upper end of the sample disc.
4. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: the sampling module is arranged on the upper sealing plate of the sample disc at one side of the sample disc and comprises a sampling needle, a sampling needle swing arm and a rotary arm motor; the first rotating motor is installed inside the shell, a sampling needle swing arm is installed on a rotating shaft of the first rotating motor, and a sampling needle is installed on the sampling needle swing arm.
5. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: the cleaning module is arranged on the sample plate upper sealing plate on one side of the sample plate and comprises a needle washing station and a needle washing bottle.
6. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: processing module installs on the sample dish of sample dish one side goes up the shrouding, processing module includes SPE column pressure head, pressure head swing arm and second rotation motor, the second rotates the motor and installs inside the casing, install the pressure head swing arm in the pivot that the second rotated the motor, SPE column pressure head is installed to pressure head swing arm upper end.
7. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: the collection module is mounted on the sample tray chassis and includes a collection trough.
8. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: the temperature control column module is arranged on the front sealing plate side of the foreign product tray and comprises a column temperature control cover plate and a column temperature control fixing groove.
9. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: the extraction advances kind module and installs in the right side of casing, the extraction advances kind module and includes high-pressure extraction pump, sampling valve, first three-way valve, second three-way valve, high-pressure reagent pump, multi-way diverter valve, first sample extraction valve, second sample extraction valve, sample transfer valve.
10. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: the operation control module comprises a touch display and a controller mainboard, the touch display is mounted at the front end of the shell, and the controller mainboard and the side sealing plate are connected inside the shell.
11. The full-automatic comprehensive pretreatment instrument for samples according to claim 1, characterized in that: the shell is further connected with a first serial port adapter, a second serial port adapter, a connector and an IC card reader of the power socket.
12. A pretreatment method of a full-automatic sample comprehensive pretreatment instrument comprises the following steps:
placing the sample tube, the extraction tube and the collection tube in a designated station of the lofting module in sequence, and setting corresponding processing methods in the operation control module in sequence;
the sampling module quantitatively sucks a sample from a sample tube in the lofting module to a designated processing station (extraction tube); before different samples are sucked, the cleaning module cleans the sampling module;
the processing module quantitatively releases the reagent to a designated processing station (extraction tube), and after incubation for a certain time, the air pump positive pressure extraction tube is started to transfer the processed target solution to the collection module; wherein, the types of the reagents are one or more; before different reagents are sucked, the cleaning module cleans the processing module;
the collection module collects and quantitatively transfers the target solution to a quantitative ring of a sample injection valve in the extraction sample injection module; cleaning the collection module after transferring;
the extraction and sample introduction module is used for carrying out on-line further treatment on the target solution transferred by the collection module, including further purification, extraction, enrichment, desorption and separation, and the treated solution can be directly transferred into an on-line analysis column.
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| CN202010265533.8A CN111624277A (en) | 2020-04-07 | 2020-04-07 | Full-automatic comprehensive sample pretreatment instrument |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112729988A (en) * | 2020-12-29 | 2021-04-30 | 石家庄正道动物药业有限公司 | Quality detection sampling device for traditional Chinese veterinary medicine dichroine and working method thereof |
| CN112946133A (en) * | 2021-02-04 | 2021-06-11 | 科诺美(北京)科技有限公司 | Application method of biological sample pretreatment system |
| CN113189255A (en) * | 2021-05-11 | 2021-07-30 | 苏州艾迪迈医疗科技有限公司 | Full-automatic sample pretreatment device and treatment method |
| WO2022166766A1 (en) * | 2021-02-02 | 2022-08-11 | 药明激创(佛山)生物科技有限公司 | Liquid workstation for solid-phase extraction and chip array sample application |
| CN115015433A (en) * | 2022-06-29 | 2022-09-06 | 江南大学 | Method for automatically detecting pesticide residues in tea |
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Cited By (5)
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| CN112729988A (en) * | 2020-12-29 | 2021-04-30 | 石家庄正道动物药业有限公司 | Quality detection sampling device for traditional Chinese veterinary medicine dichroine and working method thereof |
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| CN112946133A (en) * | 2021-02-04 | 2021-06-11 | 科诺美(北京)科技有限公司 | Application method of biological sample pretreatment system |
| CN113189255A (en) * | 2021-05-11 | 2021-07-30 | 苏州艾迪迈医疗科技有限公司 | Full-automatic sample pretreatment device and treatment method |
| CN115015433A (en) * | 2022-06-29 | 2022-09-06 | 江南大学 | Method for automatically detecting pesticide residues in tea |
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